Electric Literature of 685115-77-9, In the chemical reaction process,reaction time,type of solvent,can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product.An updated downstream synthesis route of 685115-77-9 as follows.
To a solution of 1-(3,5-dichloropyridin-4-yl)piperidine-4-carboxamide 23 (0.10 g, 0.36 mmol) in polyphosphoric acid (5 ml.) at 80 0C was added vinylene carbonate (35 mg,0.40 mmol). The mixture was heated at 170 0C for 4 hours, cooled to r.t. and poured into water (200 ml_). The mixture was extracted with ethyl acetate (3 x 50 ml.) and the combined organic extracts were washed with water (100 ml_), a saturated solution of sodium hydrogen carbonate (50 ml_), water (50 ml_), brine (50 ml_), dried (MgSO4) and concentrated under reduced pressure to furnish a colourless oil (12 mg). The crude product was purified by preparative tic on silica gel (CH2CI2, MeOH, 10:1 then hexane,EtOAc, 1 :1 ) to furnish the title compound as a white solid (13 mg, 12%), LC-MS (ESI) Rt 2.66 min, m/z 298 (100%, M+); m/z (ESI) Ci3H14CI2N3O requires 298.0508 found [M+H]+ 298.0507.
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,685115-77-9, its application will become more common.
Reference:
Patent; CANCER RESEARCH TECHNOLOGY LIMITED; McDONALD, Edward; BLAGG, Julian; PICHOWICZ, Mark; CRUMPLER, Simon Ross; WO2010/41054; (2010); A1;,
Pyridine – Wikipedia,
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